CN117380152B - Preparation method of composite mineral lithium ion adsorbent and brine lithium extraction method - Google Patents
Preparation method of composite mineral lithium ion adsorbent and brine lithium extraction method Download PDFInfo
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- CN117380152B CN117380152B CN202311214296.2A CN202311214296A CN117380152B CN 117380152 B CN117380152 B CN 117380152B CN 202311214296 A CN202311214296 A CN 202311214296A CN 117380152 B CN117380152 B CN 117380152B
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- 239000003463 adsorbent Substances 0.000 title claims abstract description 91
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 title claims abstract description 71
- 229910001416 lithium ion Inorganic materials 0.000 title claims abstract description 71
- 229910052500 inorganic mineral Inorganic materials 0.000 title claims abstract description 53
- 239000011707 mineral Substances 0.000 title claims abstract description 53
- 239000002131 composite material Substances 0.000 title claims abstract description 51
- 239000012267 brine Substances 0.000 title claims abstract description 29
- HPALAKNZSZLMCH-UHFFFAOYSA-M sodium;chloride;hydrate Chemical compound O.[Na+].[Cl-] HPALAKNZSZLMCH-UHFFFAOYSA-M 0.000 title claims abstract description 29
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 26
- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 238000000605 extraction Methods 0.000 title description 4
- 239000000843 powder Substances 0.000 claims abstract description 80
- 239000002245 particle Substances 0.000 claims abstract description 65
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 50
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 claims abstract description 44
- 238000002156 mixing Methods 0.000 claims abstract description 32
- 239000007790 solid phase Substances 0.000 claims abstract description 32
- 229910001570 bauxite Inorganic materials 0.000 claims abstract description 29
- 238000000034 method Methods 0.000 claims abstract description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000006243 chemical reaction Methods 0.000 claims abstract description 22
- 238000001035 drying Methods 0.000 claims abstract description 22
- 238000001179 sorption measurement Methods 0.000 claims abstract description 19
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 18
- 239000000440 bentonite Substances 0.000 claims abstract description 17
- 229910000278 bentonite Inorganic materials 0.000 claims abstract description 17
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 claims abstract description 17
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000001354 calcination Methods 0.000 claims abstract description 11
- 238000001914 filtration Methods 0.000 claims abstract description 10
- 238000010438 heat treatment Methods 0.000 claims abstract description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 12
- 238000001816 cooling Methods 0.000 claims description 12
- 239000008367 deionised water Substances 0.000 claims description 12
- 229910021641 deionized water Inorganic materials 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 10
- 239000011259 mixed solution Substances 0.000 claims description 8
- 230000007935 neutral effect Effects 0.000 claims description 7
- 238000004064 recycling Methods 0.000 claims description 7
- 238000000227 grinding Methods 0.000 claims description 6
- 238000004090 dissolution Methods 0.000 claims description 3
- 238000012216 screening Methods 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 230000002378 acidificating effect Effects 0.000 claims description 2
- 238000003795 desorption Methods 0.000 claims description 2
- 238000005469 granulation Methods 0.000 abstract description 10
- 230000003179 granulation Effects 0.000 abstract description 10
- 239000002994 raw material Substances 0.000 abstract description 5
- 239000003153 chemical reaction reagent Substances 0.000 abstract description 4
- 238000000975 co-precipitation Methods 0.000 abstract description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 22
- 230000001105 regulatory effect Effects 0.000 description 12
- 229910052759 nickel Inorganic materials 0.000 description 11
- 239000011734 sodium Substances 0.000 description 11
- 230000000052 comparative effect Effects 0.000 description 9
- 238000011068 loading method Methods 0.000 description 6
- 238000001878 scanning electron micrograph Methods 0.000 description 6
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 4
- VMWZRHGIAVCFNS-UHFFFAOYSA-J aluminum;lithium;tetrahydroxide Chemical compound [Li+].[OH-].[OH-].[OH-].[OH-].[Al+3] VMWZRHGIAVCFNS-UHFFFAOYSA-J 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 238000000465 moulding Methods 0.000 description 4
- 229910004298 SiO 2 Inorganic materials 0.000 description 3
- JFBZPFYRPYOZCQ-UHFFFAOYSA-N [Li].[Al] Chemical compound [Li].[Al] JFBZPFYRPYOZCQ-UHFFFAOYSA-N 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- 125000004122 cyclic group Chemical group 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 230000008929 regeneration Effects 0.000 description 3
- 238000011069 regeneration method Methods 0.000 description 3
- 238000007873 sieving Methods 0.000 description 3
- 238000002336 sorption--desorption measurement Methods 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- 239000002253 acid Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 238000005453 pelletization Methods 0.000 description 2
- 238000011085 pressure filtration Methods 0.000 description 2
- 239000011780 sodium chloride Substances 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 238000001994 activation Methods 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- ANBBXQWFNXMHLD-UHFFFAOYSA-N aluminum;sodium;oxygen(2-) Chemical compound [O-2].[O-2].[Na+].[Al+3] ANBBXQWFNXMHLD-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- QHGJSLXSVXVKHZ-UHFFFAOYSA-N dilithium;dioxido(dioxo)manganese Chemical compound [Li+].[Li+].[O-][Mn]([O-])(=O)=O QHGJSLXSVXVKHZ-UHFFFAOYSA-N 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 238000009616 inductively coupled plasma Methods 0.000 description 1
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 description 1
- 229910003002 lithium salt Inorganic materials 0.000 description 1
- 159000000002 lithium salts Chemical class 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910001388 sodium aluminate Inorganic materials 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000007725 thermal activation Methods 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
- B01J20/08—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04 comprising aluminium oxide or hydroxide; comprising bauxite
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0248—Compounds of B, Al, Ga, In, Tl
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0274—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04 characterised by the type of anion
- B01J20/0288—Halides of compounds other than those provided for in B01J20/046
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
- B01J20/041—Oxides or hydroxides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
- B01J20/043—Carbonates or bicarbonates, e.g. limestone, dolomite, aragonite
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
- B01J20/046—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium containing halogens, e.g. halides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/103—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate comprising silica
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/12—Naturally occurring clays or bleaching earth
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B26/00—Obtaining alkali, alkaline earth metals or magnesium
- C22B26/10—Obtaining alkali metals
- C22B26/12—Obtaining lithium
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/22—Treatment or purification of solutions, e.g. obtained by leaching by physical processes, e.g. by filtration, by magnetic means, or by thermal decomposition
- C22B3/24—Treatment or purification of solutions, e.g. obtained by leaching by physical processes, e.g. by filtration, by magnetic means, or by thermal decomposition by adsorption on solid substances, e.g. by extraction with solid resins
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4806—Sorbents characterised by the starting material used for their preparation the starting material being of inorganic character
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
Abstract
The invention discloses a preparation method of a composite mineral lithium ion adsorbent and a method for extracting lithium from brine, which relate to the technical field of lithium ion adsorbents in brine and aim to solve the problem that AlCl is adopted in the prior art 3 At least one of the problems of large consumption of chemical reagents, poor economy and obvious reduction of adsorption performance after organic granulation of the raw materials of the synthetic aluminum adsorbent by adopting a coprecipitation mode of NaOH and LiCl. In the method, bauxite powder, bentonite powder, naOH powder and Na powder are mixed 2 CO 3 Mixing the powder, granulating to form balls, and then carrying out calcination reaction to obtain first particles; mixing and filtering the first particles and ethyl orthosilicate, and heating and reacting the first solid phase to obtain second particles; alCl is added 3 Mixing with LiCl, water and second particles, adjusting the pH value twice, and drying to obtain the composite mineral lithium ion adsorbent. The invention can be used for extracting lithium from brine.
Description
Technical Field
The invention relates to the technical field of lithium ion adsorbents in brine, in particular to a preparation method of a composite mineral lithium ion adsorbent and a method for extracting lithium from brine.
Background
Currently, the main adsorbents for lithium ion adsorption in brine include ion sieve adsorbents, organic imprinting adsorbents and aluminum adsorbents.
The ion sieve adsorbent mainly comprises lithium manganate and lithium titanate adsorbents, a large amount of acid is used in the regeneration process, the environment-friendly performance is poor, and the ion sieve adsorbent has not been industrially applied at present. The organic imprinting adsorbent is prepared by grafting a group with lithium ion adsorption capacity onto the surface of a substrate material by an organic chemical method, and adsorbing lithium ions by using a functional group, so that the preparation process is complex, the consumption of regenerated acid is high, the manufacturing cost is high, and the industrial application is not facilitated. The aluminum-based adsorbent is generally lithium aluminum layered hydroxide, which is the only adsorbent used in industrialization for extracting lithium from brine by adsorption, but AlCl is mostly used as the aluminum-based adsorbent 3 Mixing and precipitating NaOH and LiCl, granulating with organic polymer, and synthesizing AlCl 3 The consumption of NaOH and LiCl is large, the economy is relatively poor, and the adsorption performance of the material is obviously reduced after the granulation in the organic process.
Disclosure of Invention
In view of the above analysis, the present invention aims to provide a method for preparing a composite mineral lithium ion adsorbent and a method for extracting lithium from brine, so as to solve the problem of adopting AlCl in the prior art 3 At least one of the problems of large consumption of chemical reagents, poor economy and obvious reduction of adsorption performance after organic granulation of the raw materials of the synthetic aluminum adsorbent by adopting a coprecipitation mode of NaOH and LiCl.
The aim of the invention is mainly achieved by the following technical scheme.
The invention provides a preparation method of a composite mineral lithium ion adsorbent, which comprises the following steps:
step 1: bauxite, bentonite, naOH and Na 2 CO 3 Grinding into powder respectively, mixing bauxite powder, bentonite powder, naOH powder and Na powder 2 CO 3 Uniformly mixing the powder to obtain first powder;
step 2: adding water into the first powder, fully mixing, granulating into balls, drying the balls to constant weight, calcining, and cooling to obtain first particles;
step 3: mixing the first particles with ethyl orthosilicate, standing, filtering to obtain a first solid phase, drying the first solid phase to constant weight, heating for reaction, and cooling to obtain second particles;
step 4: alCl is added 3 Adding LiCl into water for dissolution, and then adding second particles; and regulating the pH value to be acidic, carrying out stirring reaction, regulating the pH value to be neutral, filtering and washing after stirring, drying the washed solid phase to be constant weight, and screening the dried solid phase to obtain third particles and second powder, wherein the third particles are composite mineral lithium ion adsorbent.
Further, in step 1, bauxite powder, bentonite powder, naOH powder and Na powder 2 CO 3 The mass ratio of the powder is 1.0: (0.1-0.3): (0.2-0.5): (0.1-0.2).
Further, in step 2, the mass-to-volume ratio of the first powder to water is 1.0g: 0.2-0.3 ml.
Further, in the step 3, the standing time is 1-2 hours.
Further, in step 3, the mass-to-volume ratio of the first particles to the ethyl orthosilicate is 1g: 3-6 ml.
Further, in step 4, the second particles, liCl and AlCl 3 The mass ratio of (2) is 1: (0.05-0.2): (0.2 to 0.4); the mass volume ratio of the second particles to the deionized water is 1: 8-12 g/ml.
Further, the pH is regulated to 3-4, the reaction is stirred for 1-2 hours at room temperature, then the pH is regulated to be neutral, and the reaction is stirred for 1-2 hours.
Further, the step 4 further comprises the following steps:
adding hydrochloric acid to dissolve the second powder to obtain a mixed solution containing aluminum and lithium, wherein the mixed solution is AlCl in the step 4 3 And Al in LiCl 3+ And Li (lithium) + And (5) recycling.
The invention also provides a method for extracting lithium from brine, which is characterized by comprising the following steps:
step A: the preparation method is adopted to prepare the composite mineral lithium ion adsorbent;
and (B) step (B): and mixing the composite mineral lithium ion adsorbent with brine, and performing vibration adsorption.
Further, the step B further comprises the following steps:
step C: mixing the adsorbent after adsorbing lithium ions with water, vibrating for desorption, and drying the desorbed adsorbent to finish the reutilization of the adsorbent.
Compared with the prior art, the invention can realize at least one of the following beneficial effects.
A) The preparation method of the composite mineral lithium ion adsorbent provided by the invention adopts the prepared adsorbent as a supported lithium ion adsorbent, adopts cheap and easily available natural bauxite as a main aluminum source, adopts a solid-phase alkali-thermal-activated granulation-surface-supported combination method, realizes granulation of the adsorbent on one hand, and adopts acidolysis and double hydrolysis to carry out LiCl & 2Al (OH) on the other hand 3 ·nH 2 O is loaded on the surface of the material to prepare the formed composite mineral lithium ion adsorbent, compared with the conventional AlCl 3 Synthesis of lithium aluminum composite hydroxide, alCl by chemical reagents of NaOH and LiCl 3 The amounts of NaOH and LiCl used are significantly reduced.
B) Compared with an organic bonding granulation method of an aluminum adsorbent, the preparation method of the composite mineral lithium ion adsorbent provided by the invention adopts an inorganic granulation mode, realizes the molding of minerals, combines molding and loading, is beneficial to the extraction of lithium resources in brine and the effective utilization of mineral resources, is simple and easy to implement, has easily obtained raw materials, is low in cost and is environment-friendly.
In the invention, the technical schemes can be mutually combined to realize more preferable combination schemes. Additional features and advantages of the invention will be set forth in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention. The objectives and other advantages of the invention may be realized and attained by the embodiments of the invention particularly pointed out in the written description and drawings.
Drawings
The drawings are only for purposes of illustrating particular embodiments and are not to be construed as limiting the invention, like reference numerals being used to refer to like parts throughout the several views.
FIG. 1 is a flow chart of a method for preparing a shaped composite mineral lithium ion adsorbent according to the present invention;
FIG. 2a is an SEM image of second particles of the invention prepared according to example 3;
FIG. 2b is an SEM image of a composite mineral lithium ion adsorbent prepared according to example 3 of the invention;
FIG. 2c is an SEM image of the composite mineral lithium ion adsorbent prepared in example 3 of the invention after regeneration;
fig. 3 is an XRD spectrum of the composite mineral lithium ion adsorbent of example 3 of the present invention.
Detailed Description
The following detailed description of preferred embodiments of the invention is made in connection with the accompanying drawings, which form a part hereof, and together with the description of the embodiments of the invention, are used to explain the principles of the invention and are not intended to limit the scope of the invention.
The invention provides a preparation method of a composite mineral lithium ion adsorbent, which is shown in fig. 1, and comprises the following steps:
step 1: bauxite (natural bauxite), bentonite, naOH and Na 2 CO 3 Grinding into powder respectively, mixing bauxite powder, bentonite powder, naOH powder and Na powder 2 CO 3 Uniformly mixing the powder to obtain first powder;
step 2: adding water (such as deionized water) into the first powder, fully mixing, granulating into spheres with the diameter of 2-3 mm, drying the spheres to constant weight, placing the spheres into a nickel crucible, placing the nickel crucible into a muffle furnace for calcining reaction, and cooling for standby to obtain first particles;
step 3: mixing the first particles with ethyl orthosilicate, standing, filtering at normal pressure to obtain a first solid phase, drying the first solid phase to constant weight, placing the first solid phase in a nickel crucible for heating reaction, and cooling to obtain second particles;
step 4: alCl is added 3 And LiCl is added to water (e.g., deionized water) for dissolution, and then the second particles are added; regulating pH to 3-4, stirring at room temperature for reaction for 1-2 hr, regulating pH to neutrality, stirring for 1-2 hr, filtering, washing, and fixingAnd drying the phase to constant weight, and screening the dried solid phase to obtain third particles and second powder, wherein the third particles are composite mineral lithium ion adsorbent.
The principle of the preparation method for preparing the composite mineral lithium ion adsorbent is as follows:
aluminum ore-NaAlO 2 +LiCl+H + bauxite-LiCl 2Al (OH) 3 ·nH 2 O+NaCl
Aluminum ore-NaAlO 2 +LiCl+AlCl 3 +nH 2 O→bauxite-LiCl 2Al (OH) 3 ·nH 2 O+NaCl
Compared with the prior art, the preparation method of the composite mineral lithium ion adsorbent provided by the invention has the advantages that the prepared adsorbent is a supported lithium ion adsorbent, the cheap and easily obtained natural bauxite is used as a main aluminum source, and the combination method of solid-phase alkali thermal activation granulation and surface loading is adopted, so that the granulation of the adsorbent is realized, and meanwhile, liCl 2Al (OH) is subjected to acidolysis and double hydrolysis 3 ·nH 2 O is loaded on the surface of the material to prepare the formed composite mineral lithium ion adsorbent, compared with the conventional AlCl 3 Synthesis of lithium aluminum composite hydroxide, alCl by chemical reagents of NaOH and LiCl 3 The amounts of NaOH and LiCl used are significantly reduced.
In addition, compared with the organic binding granulation method of the aluminum adsorbent, the method adopts an inorganic granulation mode, realizes the molding of minerals, combines molding and loading, is beneficial to the extraction of lithium resources in brine and the effective utilization of mineral resources, is simple and easy to implement, has easily obtained raw materials, low cost and is environment-friendly.
Specifically, in the step 1, bauxite, bentonite, naOH and Na2CO are mixed 3 After crushing, mixing, and sufficiently reducing the particle size, so that the subsequent (i.e. step 2) forming and calcining are facilitated. In the step 2, the bauxite particles can be heated and activated by adopting solid phase mixingConversion of aluminium sources to sodium aluminate (NaAlO) 2 ) The method comprises the steps of carrying out a first treatment on the surface of the In the step 3, active SiO is loaded on the surface of the first particles 2 Increase the specific surface area of the first particles and reduce NaAlO 2 Shedding, strengthening the subsequent active ingredient (i.e., liCl 2Al (OH) 3 ·nH 2 O) generation and loading.
In order to be able to ensure sufficient contact of the bauxite powder with the sodium hydroxide powder, the particle size of the bauxite powder in the above step 1 is, for example, 100 to 120 mesh. The particle size of the bauxite particles is limited in the range, so that on one hand, the specific surface area of the bauxite particles can be ensured, the contact between the bauxite particles and sodium hydroxide powder is enhanced, and on the other hand, the bauxite powder can be ensured to have enough granularity, and the subsequent adsorption and separation are convenient.
Notably, in order to be able to ensure adequate activation of the bauxite particles, in step 1, for example, the bauxite powder, bentonite powder, naOH powder and Na 2 CO 3 The mass ratio of the powder is 1.0: (0.1-0.3): (0.2-0.5): (0.1-0.2).
In order to ensure sufficient calcination reaction of bauxite particles and calcination reaction rate, the calcination reaction is performed by heating to 400 to 600 ℃ at a heating rate of 4 to 6 ℃/min for 1 to 2 hours, for example, in the step 2.
In order to achieve the pelletizing effect and ensure the pelletizing stability, in the step 2, the mass-to-volume ratio of the first powder to the water is 1.0g: 0.2-0.3 ml.
Due to the surface loading of active SiO 2 The first particles of (2) can be separated by standing, so as to improve the surface loading of active SiO 2 In step 3, the standing time is, for example, 1 to 2 hours.
Likewise, to be able to ensure the activity SiO 2 In the step 3, the mass-volume ratio of the first particles to the tetraethyl orthosilicate is 1g: 3-6 ml.
The second particles, liCl and AlCl 3 The mass ratio of (2) is that the composite mineral lithium ion adsorbent is recoveredOne of the influencing parameters of the yield, illustratively, in step 4 above, the second particles, liCl and AlCl 3 The mass ratio of (2) is 1: (0.05-0.2): (0.2 to 0.4); correspondingly, the mass volume ratio of the second particles to the deionized water is 1: 8-12 g/ml.
In order to be able to secure the drying effect and the drying efficiency, the drying temperature is 50 to 70 c (e.g., 50 c, 53 c, 55 c, 59 c, 64 c, 68 c or 70 c) in the above-mentioned step 2, step 3 and step 4.
It is noted that the second powder in the step 4 is an unloaded product in the reaction process, and the main component thereof is aluminum lithium hydroxide, so as to improve the utilization rate of the second powder and the raw materials in the whole preparation process, and realize the recycling of the added aluminum salt and lithium salt, and the step 4 further comprises the following steps:
adding 0.1mol/L hydrochloric acid to dissolve the second powder to obtain a mixed solution containing aluminum and lithium, and returning to the step 4 to serve as AlCl 3 And Al in LiCl 3+ And Li (lithium) + And (5) recycling.
The invention also provides a method for extracting lithium from brine, which comprises the following steps:
step A: the preparation method is adopted to prepare the composite mineral lithium ion adsorbent;
and (B) step (B): mixing the composite mineral lithium ion adsorbent and brine in a conical flask, wherein the mass-volume ratio of the composite mineral lithium ion adsorbent to the brine is 1: 40-60 g/ml, vibrating and adsorbing for 5-7 h at room temperature, measuring the concentration of lithium ions in the adsorbed brine by adopting an inductively coupled plasma emission spectrometer (ICP-OES), and calculating the adsorption quantity of the adsorbent to the lithium ions in the brine.
In order to improve the utilization rate of the composite mineral lithium ion adsorbent, the step B further comprises the following steps:
step C: mixing the adsorbent after adsorbing lithium ions with deionized water, vibrating and desorbing for 5-7 hours, and drying the desorbed adsorbent to finish the reutilization of the adsorbent.
Examples of the present invention are further described below, wherein the brine used in the examples below has a lithium ion concentration of 60.50mg/L.
Example 1
The embodiment provides a preparation method of a composite mineral lithium ion adsorbent, which comprises the following steps:
step 1: natural bauxite, bentonite, naOH and Na 2 CO 3 Grinding into powder respectively, and mixing to obtain first powder.
Wherein, natural bauxite, bentonite, naOH and Na 2 CO 3 The mass ratio of (2) is 1.0:0.2:0.4:0.15.
step 2: the first powder and deionized water were mixed in an amount of 1.0g: and (3) fully mixing 0.25mL, granulating into spheres with the diameter of 2-3 mm, drying to constant weight at 60 ℃, placing in a nickel crucible, calcining at 500 ℃ in a muffle furnace, and cooling for 1h for standby to obtain first particles.
Step 3: the first particles were admixed with ethyl orthosilicate in an amount of 1.0g:5.0ml of the mixture is mixed, stirred and kept stand for 1h, the first solid phase is obtained after normal pressure filtration, the first solid phase is dried to constant weight and is placed in a nickel crucible, the nickel crucible is calcined in a muffle furnace at 500 ℃, the reaction time is 1h, the cooling is carried out for standby, and the second particles are obtained after cooling.
Step 4: alCl is added 3 And LiCl are dissolved in deionized water, and second particles, liCl and AlCl are added 3 The mass ratio of (2) is 1:0.05:0.2. the pH is regulated to 3-4, and the reaction is stirred for 2 hours at room temperature. And continuously regulating the pH to be neutral, stirring for 2 hours, filtering the washed solid phase, drying the solid phase to constant weight at 60 ℃, and sieving the obtained solid phase to obtain third particles and second powder. The third particles are formed composite mineral lithium ion adsorbent, the second powder is an unloaded product in the reaction process, and the main component of the second powder is aluminum lithium hydroxide.
Step 5: and (3) adding 0.1mol/L hydrochloric acid to dissolve the second powder to obtain a mixed solution containing aluminum and lithium, and returning to the step (4) for recycling.
Example 2
The embodiment provides a preparation method of a composite mineral lithium ion adsorbent, which comprises the following steps:
step 1: natural bauxite, bentonite, naOH and Na 2 CO 3 Grinding into powder respectively, and mixing to obtain first powder.
Wherein, natural bauxite, bentonite, naOH and Na 2 CO 3 The mass ratio of (2) is 1.0:0.25:0.5:0.2.
step 2: the first powder and deionized water were mixed in an amount of 1.0g: and (3) fully mixing 0.30mL, granulating into spheres with the diameter of 2-3 mm, drying to constant weight at 60 ℃, placing in a nickel crucible, calcining at 550 ℃ in a muffle furnace, and cooling for 2h for standby to obtain first particles.
Step 3: the first particles were admixed with ethyl orthosilicate in an amount of 1.0g:6.0ml of the mixture is mixed, stirred and kept stand for 1.5h, the first solid phase is obtained after normal pressure filtration, the first solid phase is dried to constant weight and is placed in a nickel crucible, the nickel crucible is calcined in a muffle furnace at 500 ℃ for 1h, and the second particles are obtained after cooling.
Step 4: alCl is added 3 And LiCl are dissolved in deionized water, and second particles, liCl and AlCl are added 3 The mass ratio of (2) is 1:0.2:0.4. the pH is regulated to 3-4, and the reaction is stirred for 2 hours at room temperature. And continuously regulating the pH to be neutral, stirring for 2 hours, filtering the washed solid phase, drying the solid phase to constant weight at 60 ℃, and sieving the obtained solid phase to obtain third particles and second powder. The third particles are formed composite mineral lithium ion adsorbent, the second powder is an unloaded product in the reaction process, and the main component of the second powder is aluminum lithium hydroxide.
Step 5: and (3) adding 0.1mol/L hydrochloric acid to dissolve the second powder to obtain a mixed solution containing aluminum and lithium, and returning to the step (4) for recycling.
Example 3
The embodiment provides a preparation method of a composite mineral lithium ion adsorbent, which comprises the following steps:
step 1: natural bauxite, bentonite, naOH and Na 2 CO 3 Grinding into powder respectively, and mixing to obtain first powder.
Wherein, natural bauxite, bentonite, naOH andNa 2 CO 3 the mass ratio of (2) is 1.0:0.15:0.4:0.1.
step 2: the first powder and deionized water were mixed in an amount of 1.0g: and (3) fully mixing 0.2mL, granulating into spheres with the diameter of 2-3 mm, drying to constant weight at 60 ℃, placing in a nickel crucible, calcining at 600 ℃ in a muffle furnace, and cooling for 1-2 h to obtain first particles.
Step 3: the first particles were admixed with ethyl orthosilicate in an amount of 1.0g:8.0ml of the mixture is stirred, mixed and kept stand for 2.0h, the mixture is filtered at normal pressure to obtain a first solid phase, the first solid phase is dried to constant weight, and the first solid phase is placed in a nickel crucible for heating reaction, and cooled to obtain second particles.
Step 4: alCl is added 3 And LiCl are dissolved in deionized water, and second particles, liCl and AlCl are added 3 The mass ratio of (2) is 1:0.1: and 0.3, regulating the pH value to 3-4, and stirring and reacting for 1h at room temperature. And continuously regulating the pH to be neutral, stirring for 2 hours, filtering the washed solid phase, drying the solid phase to constant weight at 60 ℃, and sieving the obtained solid phase to obtain third particles and second powder. The third particles are formed composite mineral lithium ion adsorbent, the second powder is an unloaded product in the reaction process, and the main component of the second powder is aluminum lithium hydroxide.
Step 5: and (3) adding 0.1mol/L hydrochloric acid to dissolve the second powder to obtain a mixed solution containing aluminum and lithium, and returning to the step (4) for recycling.
For this example, FIG. 2a is an SEM image of a second particle of the invention prepared according to example 3; FIG. 2b is an SEM image of a composite mineral lithium ion adsorbent prepared according to example 3 of the invention;
FIG. 2c is an SEM image of the composite mineral lithium ion adsorbent prepared in example 3 of the invention after regeneration;
fig. 3 is an XRD spectrum of the composite mineral lithium ion adsorbent of example 3 of the present invention.
Example 4
The embodiment provides a method for extracting lithium from brine, which comprises the following steps:
step A: the preparation method of the example 1 is adopted to prepare the composite mineral lithium ion adsorbent;
and (B) step (B): weighing 1.0g of adsorbent, mixing with 50ml of brine in a conical flask, and vibrating and adsorbing at room temperature for 6 hours, wherein the adsorption quantity of lithium ions is 2.06mg/g after detection;
step C: through 5 times of cyclic adsorption-desorption, the adsorption quantity of the adsorbent to lithium ions is 1.94mg/g, which proves that the composite mineral lithium ion adsorbent has good regenerability.
Example 5
The embodiment provides a method for extracting lithium from brine, which comprises the following steps:
step A: the preparation method of the example 2 is adopted to prepare the composite mineral lithium ion adsorbent;
and (B) step (B): weighing 1.0g of adsorbent, mixing with 50ml of brine in a conical flask, and vibrating and adsorbing at room temperature for 6 hours, wherein the lithium ion adsorption amount is 2.86mg/g after detection;
step C: through 5 times of cyclic adsorption-desorption, the adsorption quantity of the adsorbent to lithium ions is 2.68mg/g, which proves that the composite mineral lithium ion adsorbent has good regenerability.
Example 6
The embodiment provides a method for extracting lithium from brine, which comprises the following steps:
step A: the preparation method of the example 3 is adopted to prepare the composite mineral lithium ion adsorbent;
and (B) step (B): weighing 1.0g of adsorbent, mixing with 50ml of brine in a conical flask, and vibrating and adsorbing at room temperature for 6 hours, wherein the adsorption quantity of lithium ions is 2.36mg/g after detection;
step C: through 5 times of cyclic adsorption-desorption, the adsorption quantity of the adsorbent to lithium ions is 2.24mg/g, which proves that the composite mineral lithium ion adsorbent has good regenerability.
Comparative example 1
The preparation method of comparative example 1 was substantially the same as in example 3, except that NaOH was not added in step 1, and the adsorbent of comparative example 1 was examined to have an adsorption amount of 0.56mg/g for lithium ions.
Comparative example 2
The preparation method of comparative example 2 was substantially the same as in example 3 except that in step 3, the first particles were not reacted with tetraethyl orthosilicate, and the adsorption amount of lithium ions by the adsorbent of comparative example 2 was detected to be 0.72mg/g.
Comparative example 3
The preparation of comparative example 2 is essentially the same as that of example 3, except that AlCl is not added in step 4 3 The solution, as detected, the adsorbent of comparative example 3 had an adsorption amount of lithium ions of 0.52mg/g.
The present invention is not limited to the above-mentioned embodiments, and any changes or substitutions that can be easily understood by those skilled in the art within the technical scope of the present invention are intended to be included in the scope of the present invention.
Claims (6)
1. The preparation method of the composite mineral lithium ion adsorbent is characterized by comprising the following steps of:
step 1: bauxite, bentonite, naOH and Na 2 CO 3 Grinding into powder respectively, mixing bauxite powder, bentonite powder, naOH powder and Na powder 2 CO 3 Uniformly mixing the powder to obtain first powder;
step 2: adding water into the first powder, fully mixing, granulating into balls, drying the balls to constant weight, calcining, and cooling to obtain first particles;
step 3: mixing the first particles with ethyl orthosilicate, standing, filtering to obtain a first solid phase, drying the first solid phase to constant weight, heating for reaction, and cooling to obtain second particles;
step 4: alCl is added 3 Adding LiCl into water for dissolution, and then adding second particles; adjusting the pH to be acidic, stirring for reaction, then adjusting the pH to be neutral, filtering and washing after stirring, drying the washed solid phase to be constant weight, and screening the dried solid phase to obtain third particles and second powder, wherein the third particles are composite mineral lithium ion adsorbent;
in the step 1, bauxite powder, bentonite powder, naOH powder and Na powder 2 CO 3 The mass ratio of the powder is 1.0: (0.1-0).3)：(0.2～0.5)：(0.1～0.2)；
In the step 2, the mass volume ratio of the first powder to the water is 1.0g: 0.2-0.3 ml;
in the step 3, the mass volume ratio of the first particles to the tetraethoxysilane is 1g: 3-6 ml;
in the step 4, the second particles, liCl and AlCl 3 The mass ratio of (2) is 1: (0.05-0.2): (0.2 to 0.4); the mass volume ratio of the second particles to the deionized water is 1: 8-12 g/ml.
2. The method for preparing a composite mineral lithium ion adsorbent according to claim 1, wherein in the step 3, the standing time is 1 to 2 hours.
3. The method for preparing a composite mineral lithium ion adsorbent according to claim 1, wherein the pH is adjusted to 3 to 4, the reaction is stirred at room temperature for 1 to 2 hours, and then the pH is adjusted to neutral, and the reaction is stirred for 1 to 2 hours.
4. The method for preparing a composite mineral lithium ion adsorbent according to claim 1, wherein the step 4 further comprises the following steps:
adding hydrochloric acid to dissolve the second powder to obtain a mixed solution containing aluminum and lithium, wherein the mixed solution is taken as AlCl in the step 4 3 And Al in LiCl 3+ And Li (lithium) + And (5) recycling.
5. The method for extracting lithium from brine is characterized by comprising the following steps of:
step A: preparing a composite mineral lithium ion adsorbent by the preparation method according to any one of claims 1 to 4;
and (B) step (B): and mixing the composite mineral lithium ion adsorbent with brine, and performing vibration adsorption.
6. The method for extracting lithium from brine according to claim 5, wherein the step B further comprises the steps of:
step C: mixing the adsorbent after adsorbing lithium ions with water, vibrating for desorption, and drying the desorbed adsorbent to finish the reutilization of the adsorbent.
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